CN107723820A - Modified graphene oxide regenerated cellulose composite fibre and preparation method thereof - Google Patents
Modified graphene oxide regenerated cellulose composite fibre and preparation method thereof Download PDFInfo
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- CN107723820A CN107723820A CN201710884919.5A CN201710884919A CN107723820A CN 107723820 A CN107723820 A CN 107723820A CN 201710884919 A CN201710884919 A CN 201710884919A CN 107723820 A CN107723820 A CN 107723820A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
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Abstract
The present invention relates to a kind of modified graphene oxide regenerated cellulose composite fibre and preparation method thereof, the regenerated cellulose composite fibre includes：Regenerated cellulose pulp treatment fluid 85~99%；Modified graphene oxide solution 0.1~15%；The ratio between solid content of modified graphene oxide is 100 in the solid content of cellulose and modified graphene oxide solution in the regenerated cellulose pulp treatment fluid：0.01~5.By preparing modified graphene oxide solution, and using microcapsules technology processing modified graphene oxide solution, modified graphene oxide dispersiveness is improved, is finally prepared using regenerated cellulose spinning technique.The modified graphene oxide regenerated cellulose composite fibre, on the basis of regenerated celulose fibre originality energy is ensured, it is set to have given play to the performances such as the excellent antibacterial of modified graphene oxide, anti-mite, far infrared, uvioresistant, its feature is water-fastness, it is not required to independent aftertreatment technology, safety and environmental protection, better meet requirement of the current people to feature, comfortableness, healthy textile.
Description
Technical field
The invention belongs to material of regenerated cellulose technical field, and it is compound to be related to a kind of modified graphene oxide regenerated cellulose
Fiber and preparation method thereof.
Background technology
Regenerated celulose fibre is a kind of relatively broad cellulose fibre of purposes, itself have good mechanical property,
Hygroscopicity, but do not have feature.Traditional functional regenerated cellulose fibre is mainly by fine in regenerated cellulose
Auxiliary agent is added in dimension or by being realized to fibre modification, and regenerated celulose fibre prepared by this method, its function
Property it is not water-fastness, pollute more serious caused by post processing, therefore regenerated celulose fibre is applied by a definite limitation.
Graphene is a kind of two-dimensional material for having carbon atom to be formed by hexagonal array, table of the graphene oxide in graphene
Layer has the modification of the oxy radicals such as carboxyl, epoxy radicals, hydroxyl.Due to graphene oxide, preparation technology is simpler, the cost of raw material
It is cheap, while graphene oxide is less susceptible to reunite compared with graphene in practical operation, therefore can be widely applied to extensive
In industrial production.
In the prior art, CN103046151A discloses a kind of graphene blending regeneration cellulose fiber, and it utilizes and aoxidizes stone
Black alkene solution mixes with regenerated cellulose solution, be molded by viscose glue wet spinning technology after, then be prepared through reduction.The party
The viscose rayon that method obtains slightly improves in terms of intensity, and its dry fracture strength is up to 2.62cN/dtex, wet breaking strength
Reach 1.54cN/dtex.But used in this method and first prepare graphene oxide regenerated celulose fibre, the method then restored
Graphene regenerated celulose fibre is prepared, may be insufficient in the presence of reducing, and produce the problems such as reducing waste liquid.
A kind of preparation method of viscose rayon is disclosed in patent document CN104328523A, specially to viscose or
The non-graphene oxide that the number of plies is not higher than 10 layers is introduced in viscose semi-finished product, the viscose rayon of acquisition has in terms of fracture strength
Significantly lifted.But this method uses alkali, acid, water washing graphene during preparing graphene, may produce extra waste liquid,
And after disperseing during preparation graphene aqueous solution, if scattered insufficient, graphene particles thing can be made excessive, generation is reunited again
Phenomenon, causes difficulty in spinning, the problems such as blocking spinneret orifice.
The content of the invention
In view of the shortcomings of the prior art, a kind of modified graphene oxide regenerated cellulose composite fibre of offer of the invention and
Its preparation method.Modified graphene oxide solution is handled by preparing modified graphene oxide solution, and using microcapsules technology,
Modified graphene oxide dispersiveness is improved, it is fine finally to prepare the regeneration with prominent antibacterial functions using rayon spinning technique
Plain composite fibre is tieed up, extends the application of regenerated celulose fibre.
The purpose of the present invention is achieved through the following technical solutions：
The invention provides a kind of modified graphene oxide regenerated cellulose composite fibre, including following mass fraction is each
Component：
Regenerated cellulose pulp treatment fluid 85~99%；
Modified graphene oxide solution 0.1~15%；
The solid content of cellulose and modified oxygen in modified graphene oxide solution in the regenerated cellulose pulp treatment fluid
The ratio between solid content of graphite alkene is 100：0.01~5.
Preferably, the concentration of modified graphene oxide is 1~10mg/ml in the modified graphene oxide solution.
Preferably, the preparation method of the modified graphene oxide solution comprises the following steps：
S1, modified graphene oxide powder is dissolved in deionized water, is configured to the aqueous solution, then add modifying agent and alkali
Property reagent, solution is adjusted to neutral or alkalescent, is ultrasonically treated, is reunited with reducing, reduces modified graphene oxide
Grain size；
S2, by through step S1 processing after solution using microcapsules technology processing, you can.
Preferably, in step S1, the addition of the modifying agent and alkaline reagent is respectively the 1% of solution weight.
Preferably, the modified graphene oxide raw powder's production technology uses Hummers methods, specifically includes following step
Suddenly：
A1, into reaction bulb add 98% dense H2SO4；Then graphite powder and NaNO are weighed respectively3It is added to reaction bulb
In, stir 30min；
A2, KMnO4 is added into reaction bulb again, controlling reaction temperature is not higher than 25 DEG C, stirs 15min；Then it is warming up to
30~40 DEG C, continue to stir 1h；
A3, stirring terminate temperature being warming up to 90 DEG C, add deionized water and H2O2Reacted；
After A4, reaction terminate, the solution in reaction bulb is ultrasonically treated, then filters, wash, dry, crush, obtain
To modified graphene oxide powder.
Preferably, the modifying agent is in polyvinyl alcohol, polyethylene glycol, sodium lignin sulfonate, polyethylene pyrrole network alkanone
It is one or more of；The alkaline reagent is ammoniacal liquor, potassium hydroxide, sodium hydroxide, malononitrile sulfonate, one kind in sylvite or several
Kind.
Preferably, in step S1, the particle diameter of the modified graphene oxide powder is less than 5 μm；In step S2, through microcapsules
The microcapsules diameter of particle of gained is less than 3 μm after based process.The particle diameter of the modified graphene oxide powder is unsuitable excessive, no
Graphene will be then caused to disperse in regenerated celulose fibre irregular, the increase of spinning difficulty.
Preferably, the regenerated cellulose pulp treatment fluid is prepared using following methods：
Regenerated cellulose pulp is mixed with sodium hydroxide solution, stirred, is then squeezed, at experienced and yellow
Reason, is produced；The mass ratio of the regenerated cellulose pulp and sodium hydroxide solution is 1:2~4；The matter of the sodium hydroxide solution
It is 20~40% to measure fraction.
Preferably, the pressure of the squeezing processing is 2~6kpa, and the squeezing time is 30min；Experienced processing is specially：Temperature
Spend for 20~25 DEG C, handle as 5~8h, then temperature rises to 30~35 DEG C, handles 2~4h；The yellow is handled：Temperature
Spend for 20~22 DEG C, handle as 30~50min, then temperature rises to 25~30 DEG C, handles 20~40min.
Present invention also offers a kind of preparation method of modified graphene oxide regenerated cellulose composite fibre, including it is following
Step：
Modified graphene oxide solution is warming up to 25~30 DEG C, is thoroughly mixed with cellulose pulp treatment fluid, will
Temperature rises to 38~40 DEG C, 10~15min of processing (this process is that microcapsules discharge the stage), then carries out spinning, produces described
Modified graphene oxide regenerated cellulose composite fibre.
Compared with prior art, the present invention has following beneficial effect：
1st, modified graphene oxide regenerated cellulose composite fibre prepared by the present invention, ensureing that regenerated celulose fibre is former
On the basis of performance, it is set to have given play to the excellent anti-microbial property of modified graphene oxide, its feature is water-fastness, after being not required to individually
Handling process, safety and environmental protection, better meet requirement of the current people to feature, comfortableness, healthy textile.
2nd, the method comprises the steps of firstly, preparing modified graphene oxide solution, secondly modified graphene oxide solution is ultrasonically treated
And microcapsules technology processing is carried out, enhance modified graphene oxide dispersiveness and reduce its agglomeration, finally by certain ratio
Example is added in regenerated cellulose pulp, and preparing modified graphene oxide regenerated cellulose using improved wet spinning technology answers
Condensating fiber.Composite fibre excellent antibacterial performance prepared by this method, wherein Escherichia coli, staphylococcus aureus, Candida albicans
Bacterium bacteriostasis rate reaches 99.9%.
3rd, graphene regenerated cellulose composite fibre prepared by this method, technique is simple to operation, and cost is cheap, economy effect
It is beneficial high, it is adapted to large-scale industrial production.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this area
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
A kind of preparation method of modified graphene oxide is present embodiments provided, is comprised the following steps：
Step 1, modified graphene oxide is prepared using Hummers methods.
200mL 98% dense H2SO4 is added into 1000 reaction bulbs；Consolidating for 5g graphite powders and 2g NaNO3 is weighed respectively
Body, add it in reaction bulb, turn on agitator stirring 30min；Stirring adds KMnO4 15g, control reaction temperature after terminating
Degree is not higher than 25 DEG C, stirs 15min；Water-bath is warming up to 30~40 DEG C, continues stir about 1h；Stirring terminates the temperature of water-bath
Degree is warming up to 90 DEG C, and 300ml deionized waters are instilled in solution；100mL 30% H2O2 is measured simultaneously, is added in solution,
Solution becomes vivid yellow from brownish black.Continue to stir 10min, solution is poured into beaker, ultrasonic 30min；Finally use
1000ml 5.5% watery hydrochloric acid filtering, is then fully filtered untill sulfate radical-free ion in filtrate with deionized water again；
Step 2：It is dried using freeze drier, obtains spongy modified graphene oxide.It will obtain modified oxidized
Graphene is put into airslide disintegrating mill crushing, and grinding time is 2~4 hours, and modified graphene oxide particle diameter D90 is less than 5 μm.
Embodiment 2
Present embodiments provide a kind of preparation method of modified graphene oxide regenerated cellulose composite fibre, concrete operations
Step is as follows：
Step 1：Modified graphene oxide powder prepared by embodiment 1 is dissolved in deionized water, configuration concentration 1mg/
The ml aqueous solution, and 1% ratio addition modifying agent and alkaline reagent, solution is adjusted to neutral or alkalescent.Then surpassed
Sound 30min~60min, makes it be uniformly dispersed；Then solution is handled using microcapsules technology, the microcapsules diameter of particle of gained
Less than 3 μm.
Step 2：Prepare regenerated cellulose pulp treatment fluid：500g regenerated cellulose pulps are weighed, according to mass ratio 1:(2
~4) it is that 20%~40% sodium hydroxide solution mixes with mass fraction, mixer stirring 60min, is thoroughly mixed it；By its
It is put into squeezer and squeezes, set pressure as 2~6kpa, the squeezing time is 30min；Pulp is subjected to experienced processing, experienced temperature
Spend for 20~25 DEG C, the time is 5~8h, temperature is risen into 30~35 DEG C, ageing time is 2~4h；Carried out after the completion of experienced yellow
Change, 20~22 DEG C of yellow temperature, 30~50min of yellow time；Then temperature is risen to 25~30 DEG C, the yellow time 20~
40min。
Step 3：Modified graphene oxide solution prepared by step 1 is warming up to 25~30 DEG C, prepared with step 2
Regenerated cellulose pulp treatment fluid is sufficiently mixed, and mixer mixing time is 30~60min, temperature is risen into 38~40 DEG C, place
10~15min is managed, the weight/mass percentage composition of the modified graphene oxide solution and regenerated cellulose pulp treatment fluid is respectively
15% and 85%, the ratio of cellulose solid content wherein in modified graphene oxide solid content and regenerated cellulose pulp treatment fluid
For 5%：1；The cellulose pulp most prepared at last carries out spinning, prepares modified graphene oxide regenerated cellulose composite fibre.
Embodiment 3
Present embodiments provide a kind of preparation method of modified graphene oxide regenerated cellulose composite fibre, concrete operations
Step is substantially the same manner as Example 2, the difference is that only：In step 1, configuration concentration is the 5mg/ml aqueous solution；Step 3
In, the weight/mass percentage composition of the modified graphene oxide solution and regenerated cellulose pulp treatment fluid is respectively 5% and 95%,
The ratio of cellulose solid content is 2% wherein in modified graphene oxide solid content and regenerated cellulose pulp treatment fluid：1.
Embodiment 4
Present embodiments provide a kind of preparation method of modified graphene oxide regenerated cellulose composite fibre, concrete operations
Step is substantially the same manner as Example 2, the difference is that only：In step 1, configuration concentration is the 10mg/ml aqueous solution；Step
In three, the weight/mass percentage composition of the modified graphene oxide solution and regenerated cellulose pulp treatment fluid be respectively 1% and
99%, wherein the ratio of cellulose solid content is in modified graphene oxide solid content and regenerated cellulose pulp treatment fluid
0.01%：1.
Comparative example 1
This comparative example provides a kind of preparation method of modified graphene oxide regenerated cellulose composite fibre, concrete operations
Step is substantially the same manner as Example 2, the difference is that only：In step 1, this comparative example does not carry out microcapsules technology to solution
Processing.
Comparative example 2
This comparative example provides a kind of preparation method of modified graphene oxide regenerated cellulose composite fibre, concrete operations
Step is substantially the same manner as Example 2, the difference is that only：Step 3 is：Modified graphene oxide prepared by step 1 is molten
Liquid is warming up to 25~30 DEG C, and the regenerated cellulose pulp treatment fluid prepared with step 2 is sufficiently mixed, and mixer mixing time is
30~60min, spinning is then carried out, produce the modified graphene oxide regenerated cellulose composite fibre.
Comparative example 3
This comparative example provides a kind of preparation method of modified graphene oxide regenerated cellulose composite fibre, concrete operations
Step is substantially the same manner as Example 2, the difference is that only：In step 3, the modified graphene oxide solution is fine with regeneration
Tie up plain pulp treatment fluid to be sufficiently mixed, after mixer stirring, temperature is risen to 30~32 DEG C, handles 20~25min.
Comparative example 4
This comparative example provides a kind of preparation method of graphene regenerated cellulose composite fibre, concrete operation step and reality
It is essentially identical to apply example 2, the difference is that only：In step 1, the raw material that this contrast uses is non-graphene oxide powder.
Comparative example 5
This comparative example provides a kind of preparation method of modified graphene oxide regenerated cellulose composite fibre, concrete operations
Step is substantially the same manner as Example 2, the difference is that only：In step 1, the modified graphene oxide powder of this contrast use
To be prepared by Brodie methods.
Compliance test result：
Modified graphene oxide regenerated cellulose composite fibre prepared by embodiment 2-4 and comparative example 1-4 carries out performance
Test, its result are as shown in table 1.
Table 1
Concrete application approach of the present invention is a lot, and described above is only the preferred embodiment of the present invention.More than it should be pointed out that
Embodiment is merely to illustrate the present invention, and the protection domain being not intended to limit the invention.For the common skill of the art
For art personnel, under the premise without departing from the principles of the invention, some improvement can also be made, these improvement also should be regarded as this hair
Bright protection domain.
Claims (10)
1. a kind of modified graphene oxide regenerated cellulose composite fibre, it is characterised in that include each group of following mass fraction
Point：
Regenerated cellulose pulp treatment fluid 85~99%；
Modified graphene oxide solution 0.1~15%；
The solid content of cellulose and modified oxidized stone in modified graphene oxide solution in the regenerated cellulose pulp treatment fluid
The ratio between solid content of black alkene is 100：0.01~5.
2. modified graphene oxide regenerated cellulose composite fibre according to claim 1, it is characterised in that the modification
The concentration of modified graphene oxide is 1~10mg/ml in graphene oxide solution.
3. modified graphene oxide regenerated cellulose composite fibre according to claim 1 or 2, it is characterised in that described
The preparation method of modified graphene oxide solution comprises the following steps：
S1, modified graphene oxide powder is dissolved in deionized water, is configured to the aqueous solution, then added modifying agent and alkalescence is tried
Agent, solution is adjusted to neutral or alkalescent, is ultrasonically treated；
S2, by through step S1 processing after solution using microcapsules technology processing, you can.
4. modified graphene oxide regenerated cellulose composite fibre according to claim 3, it is characterised in that step S1
In, the addition of the modifying agent and alkaline reagent is respectively the 1% of solution weight.
5. the modified graphene oxide regenerated cellulose composite fibre stated according to claim 3 office, it is characterised in that described to change
The preparation method of property graphene oxide powder uses Hummers methods, specifically includes following steps：
A1, into reaction bulb add 98% dense H2SO4；Then graphite powder and NaNO are weighed respectively3It is added in reaction bulb, stirs
Mix 30min；
A2, KMnO4 is added into reaction bulb again, controlling reaction temperature is not higher than 25 DEG C, stirs 15min；Then it is warming up to 30~
40 DEG C, continue to stir 1h；
A3, stirring terminate temperature being warming up to 90 DEG C, add deionized water and H2O2Reacted；
After A4, reaction terminate, the solution in reaction bulb is ultrasonically treated, then filters, wash, dry, crush, changed
Property graphene oxide powder.
6. the graphene regenerated cellulose composite fibre according to claim 3 or 4, it is characterised in that the modifying agent is
Polyvinyl alcohol, polyethylene glycol, sodium lignin sulfonate, polyethylene pyrrole network alkanone, malononitrile sulfonate, one kind in sylvite or several
Kind；The alkaline reagent is ammoniacal liquor, potassium hydroxide, the one or more in sodium hydroxide.
7. graphene regenerated cellulose composite fibre according to claim 3, it is characterised in that described to change in step S1
Property graphene oxide powder particle diameter be less than 5 μm；In step S2, the microcapsules diameter of particle of gained after microcapsules based process
Less than 3 μm.
8. modified graphene oxide regenerated cellulose composite fibre according to claim 1, it is characterised in that the regeneration
Cellulose pulp treatment fluid is prepared using following methods：
Regenerated cellulose pulp is mixed with sodium hydroxide solution, stirred, is then squeezed, experienced and yellow processing,
Produce；The mass ratio of the regenerated cellulose pulp and sodium hydroxide solution is 1:2~4；The quality of the sodium hydroxide solution
Fraction is 20~40%.
9. modified graphene oxide regenerated cellulose composite fibre according to claim 1, it is characterised in that the squeezing
The pressure of processing is 2~6kpa, and the squeezing time is 30min；Experienced processing is specially：Temperature is 20~25 DEG C, handle as 5~
8h, then temperature rise to 30~35 DEG C, handle 2~4h；The yellow is handled：Temperature is 20~22 DEG C, is handled as 30
~50min, then temperature rise to 25~30 DEG C, handle 20~40min.
A kind of 10. preparation of modified graphene oxide regenerated cellulose composite fibre according to claim any one of 1-9
Method, it is characterised in that comprise the following steps：
Modified graphene oxide solution is warming up to 25~30 DEG C, is thoroughly mixed with regenerated cellulose pulp treatment fluid, will
Temperature rises to 38~40 DEG C, handles 10~15min, then carries out spinning, produce the modified graphene oxide regenerated cellulose
Composite fibre.
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| PCT/CN2017/114698 WO2019061817A1 (en) | 2017-09-26 | 2017-12-06 | Modified graphene oxide regenerated cellulose composite fiber and preparation method therefor |
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| WO2024077723A1 (en) * | 2022-10-10 | 2024-04-18 | 南通强生新材料科技股份有限公司 | Extreme-cold-resistant graphene glove and preparation method therefor |
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| WO2019061817A1 (en) | 2019-04-04 |
| CN107723820B (en) | 2020-11-17 |
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